The invention relates to an electron detection device for use with an electron microscope such as a scanning electron microscope.
The orientation of individual crystals in a crystalline sample is of importance to researchers in determining the mechanical properties of materials. Semiconductors, metals and ceramics are examples of these materials. Electron Backscatter Diffraction (EBSD) is a technique employed using a Scanning Electron Microscope (SEM) that helps researchers determine crystal orientation and thereby realizing phases, phase boundaries and textures. The crystalline sample is tilted to a high angle relative to the horizontal plane, producing an almost grazing angle relative to the SEM electron beam. When the sample is scanned by the electron beam secondary or back scattered electrons and hazardous x-rays are emitted by the sample in a characteristic manner according to the physical laws of electron and x-ray diffraction.
Typically, an EBSD detector is interfaced with the SEM vacuum chamber on an available port, i.e. a hole in the SEM chamber wall. Low pressure is required inside the SEM chamber to allow electron interaction with the sample for various scientific applications, including, but not limited to imaging and x-ray analysis of the sample. The SEM chamber wall is the barrier that separates the vacuum environment inside the chamber and the atmosphere outside the chamber. Detectors, motion and electrical feed-thrus and other apparatus must pass through the chamber ports and also create a vacuum seal at the port. This vacuum seal can be static, i.e. the seal always touches the same area of the penetrating device and the SEM chamber port because the device does not move, or the seal can be dynamic, i.e. the area where the seal touches the device or the port changes as required by the motion of the device. If the relative motion of the device is translation along the axis the seal is referred to as being a xe2x80x9cslidingxe2x80x9d dynamic seal. If the relative motion of the device is rotation about the axis the seal is referred to as a xe2x80x9crotatingxe2x80x9d dynamic seal.
An example of a conventional EBSD detector is described in U.S. Pat. No. 5,557,104. In this case, the primary components of a commercially made, modern EBSD detector consists of six components. A phosphor front coated glass substrate is placed close to the sample, with surface parallel to the electron beam and is struck by the back scattered electrons. This phosphor substrate is usually supported in position by the mechanical components of the EBSD detector, typically a metal tube which may contain a fibre optic bundle. The interaction of the electrons with the phosphor produces visible light that is displayed in characteristic patterns and is viewed on the back side of the phosphor substrate. It is these patterns that are recognized and analyzed in determining the crystal orientations in the sample. If the tube does not contain a fibre optic bundle, a glass window, typically interspersed with lead to attenuate hazardous x-rays, is positioned further back from the sample, typically on the other end of the tube. The glass window is mechanically sealed on the far end of the tube, thus acting as part of the SEM vacuum barrier. The phosphor substrate, the metal tube (fibre optic bundle) and the glass window are inserted through the SEM chamber port and are vacuum sealed at the port. The vacuum seal is created by either a rubber O-ring around the outside of the tube or a very expensive and fragile welded metal bellows. Behind the glass window, on the atmosphere side, is positioned a low light level camera. Light from the phosphor is coupled to the camera by either a fibre optic bundle or by a lens system that focuses the light from the phosphor screen onto the camera transducer which is typically a Charge Coupled Device (CCD) which produces an electronic signal processed and output to a computer interface. The computer hardware and specialized software is used to present the pattern images on the monitor and aid in the recognition and analysis of the EBSD patterns.
The phosphor substrate and the metal tube which protrude into the SEM vacuum chamber occupy valuable space which must be shared inside the SEM vacuum chamber. Sample positioning and manipulation devices, such as the SEM stage, other detectors, such as Energy and X-ray Dispersive spectrometers, chamber scopes (sample viewing cameras), electron secondary and back scattered imaging devices all require space to operate inside and outside the SEM chamber. Most of these devices are designed with and include retraction mechanisms that remove the device from an operational position to a position where they will not interfere mechanically with other devices during their operation.
The vacuum seal around the EBSD metal tube is a dynamic seal and has potential to fault the SEM vacuum system when it is being retracted due to it""s relatively large size (typically 30 to 40 millimeters in diameter). If the vacuum system of the SEM is faulted during operation costly electron gun filaments can be destroyed and require replacement. This kind of seal is a xe2x80x9cslidingxe2x80x9d O-ring seal, because the tube translates along it""s axis, sliding through the O-ring. As the tube slides through the O-ring it carries with it small dust and debris particles which cling to the rubber O-ring between the O-ring and the sealing area on the tube. The mechanical force required to slide the tube through the O-ring is the sum of the friction force and the force from atmospheric pressure. As the tube diameter increases the contact area of the seal increases as does the required retraction force and the potential to cause a vacuum leak.
The EBSD metal tube interior has potential to cause optical interference detected as background noise of various levels by the camera. Some of the light that is emitted from the phosphor and is transmitted through the glass substrate bounces off the interior wall of the metal tube interfering with those rays of light that strike the CCD directly. Also, the lead glass window that prevents x-rays from escaping reduces the light signal detected by the camera.
In accordance with a first aspect of the present invention, an electron detection device for use with an electron microscope defining a sample chamber comprises a housing which in use is mounted to and opens into or forms part of a sample chamber of an electron microscope, a support structure attached to the detection device housing and in communication with the sample chamber in use, the support structure supporting within it a member from which depends a phosphor scintillator, the member being movable between an extended position in which the phosphor scintillator is close enough to a sample to be struck by electrons and a retracted position; a control system for controlling movement of the member; and a detector for monitoring light emitted by the phosphor scintillator in response to electron impact.
In contrast to the prior art, we avoid having to move a large metal housing in and out of the vacuum and instead only have to move the phosphor scintillator support member.
The control system can take a variety of forms but in one preferred approach includes a rotatably mounted shaft extending through a bore of the support structure to which it is sealed by a dynamic annular seal. Such a shaft can have a small diameter and thus only requires a small seal leading to considerably increased reliability over the sliding seals and bellows of the prior art and at substantially reduced cost.
Typically, the annular seal is in the form of an O-ring.
The advantage of this retraction mechanism is that in the preferred example less than xc2xd of a revolution (maximum for the chosen motor) of the motor shaft generates over 110 mm stroke of the telescoping tube (see below) which significantly improves the integrity, reliability and life of the dynamic vacuum seal. Multiple motor shaft revolutions will wear the O-ring and shorten the life of the seal.
Other examples of control systems include stepping motor(s) and controller, lead screw and motor, and cables, pulleys, springs and motor.
It is important to move the phosphor scintillator to the retracted position so that it does not interfere with other apparatus that may be used with the electron microscope. The fragile phosphor scintillator is also therefore protected from damage by other devices in motion within the sample chamber.
Preferably, the phosphor scintillator is pivoted to the member so that it can be rotated into a rest position when not in use. The advantage of this is that-the sample can be viewed through the support structure, possibly with the aid of external light sources, enabling the sample to be viewed directly by the detector without interference by the phosphor scintillator. This is useful for positioning the sample.
Conveniently, the phosphor scintillator is coupled to the member such that the movement of the member causes pivoting movement of the phosphor scintillator. However, it would also be possible to incorporate an additional actuator mechanism for pivoting the phosphor scintillator.
In a particularly preferred arrangement, the support structure and member define a telescopic arrangement. This reduces the space required for retracting the member. In this case, conveniently the member comprises a tube mounted for telescopic movement along a support member of the support structure, part of the support member being adapted to engage and pivot the phosphor scintillator as the tube moves to the retracted position.
The detector could be positioned so as to directly view the phosphor scintillator. However, there is a risk that it will receive X-rays and thus preferably the device further comprises a mirror for reflecting light from the phosphor scintillator towards the detector. This enables the detector to be positioned offset from a direct line of sight with the phosphor scintillator so that any X-rays will pass through the mirror and be absorbed by the support structure.
The support structure could in some cases form part of the electron detection device housing, for example being an integral extension of that housing. Conveniently, however, the support structure defines a wall which is sealed in use about a port of the electron microscope chamber.
When analysing the diffraction pattern obtained from the sample, it is important to know the geometrical relationship of the phosphor scintillator to the source (i.e. the point where the incident focused electron beam strikes the sample). The xe2x80x9cpattern centrexe2x80x9d is usually determined by moving the phosphor scintillator in and out along the axis of retraction and taking two patterns at different distances. The part of the pattern which does not move is effectively the xe2x80x9cpattern centrexe2x80x9d.
In accordance with a second aspect of the present invention, an electron detection device for use with an electron microscope defining a sample chamber comprises a support member from which depends a phosphor scintillator, the phosphor scintillator being movable on the support member between an active position in which the phosphor scintillator is close enough to a sample to be struck by electrons and a rest position; a control system for controlling movement of the phosphor scintillator; and a detector for monitoring light emitted by the phosphor scintillator in response to electron impact when the phosphor scintillator is in its active position, and for viewing the source when the phosphor scintillator is in its rest position.
This aspect of the invention makes use of the fact that the detector will have a sufficient depth of focus that the pattern centre can be determined even though the view with the scintillator in the rest position is slightly blurred. This assumes, of course, that the source sample is fluorescent. This provides a convenient and fast way of finding the pattern centre and calibrating the detector system without any retraction being required.
The phosphor scintillator could be mounted to the support member in a variety of ways to enable it to be moved between its two positions but particularly conveniently it is pivoted as described earlier. Nevertheless, it will be appreciated that it is not essential in this aspect of the invention for the phosphor scintillator to be mounted on a retractable support member.